Synthesis evidence

Solvothermal preparation of an electrocatalytic metalloporphyrin MOF thin film and its redox hopping charge-transfer mechanism

Ahrenholtz S.R., Epley C.C., Morris A.J. · Journal of the American Chemical Society · 2014 · 2464-2472

1 structured synthesis route

Completeness describes how fully the route could be reconstructed from the main article and supporting information.

Complete recipeSource: Main

Route 1: Solvothermal

7 · Experimental Section - CoPIZA Thin Film Synthesis

Metal precursorsCoCl2.6H2O (0.15 mmol)
Linker precursorsTCPP SAM on FTO; additional TCPP (0.05 mmol) in solvothermal mixture
SolventsDMSO for 0.1 mM TCPP SAM solution; 3.0 mL of 0.1 M pyridine/KOH aqueous solution; DMF wash
AdditivesKOH; pyridine
Atmospheresealed tube; gas atmosphere not specified
Temperature150
Time48
Substrate orientationFTO substrate; orientation not specified
Work-upPurple powder was filtered; powder and thin film were washed with DMF.
ActivationNo thermal/vacuum activation reported.
Scalability contextThin-film solvothermal deposition on FTO; no scale-up data reported.
Show 7 structured reagent records
RoleReagentAmount / concentrationSource
Otherfluorine-doped tin oxide (FTO; Hartford Glass)Not specified7 · Experimental Section - CoPIZA Thin Film Synthesis
Linkermeso-tetra-(4-carboxy)tetraphenyl porphine (TCPP; Frontier Scientific)0.05 mmol in solvothermal mixture · 0.1 mM in DMSO for SAM solution7 · Experimental Section - CoPIZA Thin Film Synthesis
Metal Sourcecobalt(II) chloride hexahydrate (CoCl2.6H2O)0.15 mmol7 · Experimental Section - CoPIZA Thin Film Synthesis
Basepotassium hydroxide (KOH)0.1 M pyridine/KOH aqueous solution7 · Experimental Section - CoPIZA Thin Film Synthesis
Additivepyridine, distilled before use0.1 M pyridine/KOH aqueous solution7 · Experimental Section - CoPIZA Thin Film Synthesis
SolventN,N-dimethylformamide (DMF)wash solvent7 · Experimental Section - CoPIZA Thin Film Synthesis
SolventDMSOTCPP/DMSO (0.1 mM)7 · Experimental Section - CoPIZA Thin Film Synthesis